反応 #2446100

反応方程式

p-Hydroxystyrene

triethylamine

ethyl acetate

→

desired resin

p-(1-(Cyclohexylethoxy)ethoxy)styrene p-Hydroxystyrene

溶媒

propylene glycol monomethyl ether acetate

反応条件

後処理

1. 1
   温度with heating
2. 2
   workup.DISTILLATIONdehydrated by vacuum distillation
3. 3
   workup.ADDITIONTo this solution, 0.35 g of pyridinium p-toluenesulfonate and 22.4 g of cyclohexane ethanol were added
4. 4
   workup.ADDITIONfurther 17.5 g of t-butyl vinyl ether was added at a slow speed
5. 5
   その他In the resulting mixture, reaction
6. 6
   洗浄washed with 150 ml each of distilled water for three times
7. 7
   workup.DISTILLATIONTherefrom, the solvent was distilled away
8. 8
   濃縮the residue was concentrated
9. 9
   workup.DISSOLUTIONThe thus obtained oil was dissolved in 100 ml of acetone
10. 10
    workup.ADDITIONpoured slowly into 2 liter of distilled water
11. 11
    その他As a result, a powdery matter separated out
12. 12
    ろ過This powdery matter was filtered off
13. 13
    その他dried

実験手順

p-Hydroxystyrene (VP-8000, produced by Nippon Soda Co., Ltd.) in an amount of 70 g was dissolved in 320 g of propylene glycol monomethyl ether acetate (PGMEA) with heating, dehydrated by vacuum distillation, and then cooled to 25° C. To this solution, 0.35 g of pyridinium p-toluenesulfonate and 22.4 g of cyclohexane ethanol were added, and further 17.5 g of t-butyl vinyl ether was added at a slow speed. In the resulting mixture, reaction was run for 5 hours at 20° C. Thereafter, the reaction solution was admixed with 0.28 g of triethylamine and 320 ml of ethyl acetate, and washed with 150 ml each of distilled water for three times. Therefrom, the solvent was distilled away, and the residue was concentrated. The thus obtained oil was dissolved in 100 ml of acetone, and poured slowly into 2 liter of distilled water. As a result, a powdery matter separated out. This powdery matter was filtered off and dried to yield 54 g of the desired resin.

出典